MEDISURE LABORATORIES PAKISTAN (Pvt.

) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
PROTOCOL OF PRODUCT
VAL-FM-003 17-12-2019
DESVEL 50MG TABLET

Page 1 of 16

PROCESS
VALIDATION
PROTOCOL OF
DESVEL 50MG
TABLET

VAL-PR-009
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
PROTOCOL OF PRODUCT
VAL-FM-003 17-12-2019
DESVEL 50MG TABLET

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Name Saba Alvi
Written By :
1) Signature &
Validation/QA Officer
Date

Name Mr.Usman Baig

Reviewed By :
2) Signature &
Sr. Manager Production
Date
s

Name Suffyan Ullah

Reviewed By :
3) Ass Manager Quality Signature &
Control Date

Name Anjum Siddiqui

Approved By :
4) Manager Quality Signature &
Assurance Date
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
PROTOCOL OF PRODUCT
VAL-FM-003 17-12-2019
DESVEL 50MG TABLET

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Table of Content

1.0 Objective
2.0 Rationale
3.0 Scope
4.0 Validation Team
5.0 Responsibilities
6.0 Product Description
7.0 List of Equipment
8.0 Bill of Raw Material
9.0 Process Flow
10.0 Dispensing Process description
11.0 Manufacturing Process Description
12.0 Filling
13.0 Quality Control Specifications
14.0 Packing Process Description
15.0 Sampling Criteria
16.0 Final Report
17.0 Recommendations
18.0 Outstanding Points
19.0 Decision
20.0 Report Approval

1.0 Objective
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
PROTOCOL OF PRODUCT
VAL-FM-003 17-12-2019
DESVEL 50MG TABLET

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To validate manufacturing process of DESVEL 50mg tablet.
2.0 Rationale
 All Critical steps of manufacturing process will be checked
 Critical Process Parameters and limits must be identified
 Assurance that the Process when performed within process limits performs as intended
 Assurance that the Process does perform consistently as intended
 In the case of any change in manufacturing steps, raw material/raw material sources,
manufacturing equipment & technology the revalidation will be carried out.
3.0 Scope
This protocol is only applicable to DESVEL 50mg tablet manufactured by Medisure
Laboratories (PVT) Limited.

4.0Validation Team

S.NO NAME DESIGNATION

01 Saba Alvi Validation/QA Officer

02 Dr. Anum Shakeel Production Officer

03 Mr. Usman Baig Sr Manager Production

04 Sufyan Ullah Asst. Manager Quality Control

05 Anjum Siddiqui Manager Quality Assurance

5.0 Responsibilities
5.1Quality Assurance:
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
PROTOCOL OF PRODUCT
VAL-FM-003 17-12-2019
DESVEL 50MG TABLET

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 Preparation, approval and training of validation protocol, review of the data compiled,
review of deviations (if any), monitoring the process as per the process parameters and for
with drawl of validation samples.
 Review of facility, equipment qualification.
 GMP compliance during
 Manufacturing process.
 Preparation of process validation summary report, review and approval

5.2Production:
 To execute the batches as per the batch manufacturing record and process validation
protocol.
 Compilation of data related to manufacturing area and furnishing the same for review.
 Review of protocol and summary report.

5.3 Quality Control:

 Raw material and packing material Analysis.
 In process and finished product samples Analysis as per the sampling plan.
 Collection and review of in process and finished product analysis data.
 Submission of data/results to Quality Assurance for review and evaluation.

6.0 Product Description

 Each film coated tablet contains: 76mg Desvenlafaxine Succinate equivalent to
Desvenlafaxine…………50mg

7.0 List of Equipment Used

S.No. Mfg. Steps Equipment
1 Mixing Ribbon Mixer
2 Sieving Sifter (Sieve no.16)
3 Blender Double cone blender
4 Compression ZP-17
8.0 Bill of Raw Material (Product formula)
Batch size: 0.3 Kg
S.No. Ingredients Qty/unit (mg) Qty/batch (kg)
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
PROTOCOL OF PRODUCT
VAL-FM-003 17-12-2019
DESVEL 50MG TABLET

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1 Desvenlafaxine Succinate 72.425 0.133
2 Coat Dry 8800 82.841 0.147
3 Lactose SD 13.734 0.024
Coating
4 HPMC 3.00 0.005
5 Titanium Dioxide 2.54 0.005
6 Talcum 1.00 0.002
7 PEG 6000 1.50 0.003
8 IPA 0.11 0.19
Molecular Weight of Desvenlafaxine Succinate = 381.47 g/mol
Molecular Weight of Desvenlafaxine = 263.38 g/mol
= 381.47⁄262.38=1.448
Label Claim = 50mg
= 50 × 1.448
Qty/unit = 72.425 mg

9.0 Process flow

 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
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PROTOCOL OF PRODUCT
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DESVEL 50MG TABLET

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10.0 Dispensing Process Description

 Material Requisition Sheet as per batch manufacturing record will be send to
warehouse from Production Department.
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
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VAL-FM-003 17-12-2019
DESVEL 50MG TABLET

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 After getting Material Requisition Sheet from production department dispensing
pharmacist will check the availability of approved material as per FEFO system.
 Before dispensing following points to be checked.

S.NO POINTS TO BE CHECKED YES NO

01 Before entering in dispensing area, all person will
follow secondary gowning procedure
02 Dispensing Pharmacist will check and verify all the
details, Materials name and code, Approved labels,
Manufacturing dates, Expiry dates and Retest date
before dispensing.
03 Dispensing Pharmacist will put ON the dispensing
booth before 15minutes of dispensing.
04 Products will be dispensed in the dispensing area by
using dispensing booth.
05 Dispensing Pharmacist will check the cleaning of
dispensing area as per the SOP of cleanness in
dispensing area.
06 Dispensing Pharmacist will check the pressure
difference on pressure guage.
07 Dispensing Pharmacist will check the temperature and
humidity in dispensing room.
08 Before starting the dispensing, Dispensing Pharmacist
will ensure that all the scoops are cleaned and dried to
avoid contamination and also ensure that all balances
are calibrated.
09 Dispensing Pharmacist will take line clearance from
the QA Officer and then start dispensing in the
presence of production officer and QA officer.
10 All issued material is transferred to dispensed material
storage area along with bill of raw material.

11.0Manufacturing Process Description

11.1 Method of Manufacturing:
Mixing

1) Add the following into polybag by passing through sieve and mix for 5 minutes.
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
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VAL-FM-003 17-12-2019
DESVEL 50MG TABLET

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Desvenlafaxine Succinate
Lactose SD
Coat Dry 8800
2) Check the weight and intimate QC for sampling and testing.
Compression

3) Check area, equipment and utensils before compression.

4) Keep the compressed tablets into a clean, dry polythene lined duly tared containers. Seal
the containers.
5) Record the weight of compressed tablets and consider it to the bulk tablet store.
6) Submit the sample of compressed tablet to QC.

11.2 Yield Check of Granules:

BATCH # T-001
S.NO. Yield Weight
1 Theoretical Yield 0.3 Kg
2 Actual Yield

BATCH # T-002
S.NO. Yield Weight
1 Theoretical Yield 0.3 Kg
2 Actual Yield

BATCH # T-003
S.NO. Yield Weight
1 Theoretical Yield 0.3 Kg
2 Actual Yield
11.3 Compression:
i) Check Area, equipment's and utensils before commencement

Yes No
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
PROTOCOL OF PRODUCT
VAL-FM-003 17-12-2019
DESVEL 50MG TABLET

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1 Area is cleaned and free from traces of previous product.

2 Operator is wearing mask, gloves and uniform properly.

3 Air Exhaust system is working.

4 Filling machine is properly labeled.

5 Collecting bucket having label

ii) Equipment Cleaning Checklist:

Cleaning
Equipment
Major Minor
Compression Machine
 
(ZP 17)
Tablet Deduster    

iii) Tablet Specification:

Appearance
Standard Compression Weight
Weight of 10 Tablet
Weight Variation
Hardness
Friability

Keep the compressed tablet into a clean, dry, polythene lined duly tared container. Seal the
containers.

iv) Yield Check of Compressed Tablet:

Record the weight of compressed tablet and transfer it to the bulk tablet store.
S.No. Gross (Kg) Tare (Kg) Net (Kg) Weight By
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
PROTOCOL OF PRODUCT
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DESVEL 50MG TABLET

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1 0.02

2 0.02

3 0.02

Submit the sample of compressed tablet to QC.

11.4 Yield Check After Compression:

BATCH # T-001
S.NO. Yield Weight
1 Theoretical Yield
2 Actual Yield

BATCH # T-002
S.NO. Yield Weight
1 Theoretical Yield
2 Actual Yield

BATCH # T-003
S.NO. Yield Weight
1 Theoretical Yield
2 Actual Yield

11.5 Coating:
i) Check Area, equipment's and utensils before commencement.
Yes No
1 Area is cleaned and free from traces of previous product.
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
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DESVEL 50MG TABLET

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2 Operator is wearing mask, gloves and uniform properly.

3 Coating Pan is Cleaned

4 Air Exhaust system is working.

5 Silver son mixer and container are cleaned.

6 Collecting bucket having label.

ii) Method (Solution Preparation):

1) Dissolve PEG 6000 in Distilled water. Check clarity of solution.
2) Dissolve HPMC in 0.1 L IPA in Silver-son mixer.
3) Add and mix vigorously Talcum and Titanium dioxide in step 8.
4) Add step 7 into step 8 and mix thoroughly.
5) Add remaining quantity of IPA in a solution and mix until a suitable solution is obtained.

iii) Coating of Tablets:

1. Transfer the tablet into coating pan with sieving for dedusting.
2. Warm the tablet to 30°C - 35°C.
3. Apply the coating solution in a way that after getting the solution, tablet get dried when
reached to bottom point.
4. Apply all solution and then check the average weight of tablets. It should be at least 5%
increase in core weight.
5. Collect the tablets in polythene lined drums and weigh.
6. Transfer the coated tablets to quarantine and inform QC to collect sample.

11.6 Yield Check After Coating

BATCH# T001
S.No. YIELD WEIGHT
1 THEORITICAL YIELD
2 ACTUAL YIELD

BATCH# T002
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
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PROTOCOL OF PRODUCT
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S.No. YIELD WEIGHT
1 THEORITICAL YIELD
2 ACTUAL YIELD

BATCH# T003
S.No. YIELD WEIGHT
1 THEORITICAL YIELD
2 ACTUAL YIELD
12.0 Packing Process Description:
 Ensure that packing Area is cleaned and free from left over of previous product/batch.
 Note down the temperature and humidity of the packing area.
 Ensure that the area is certified from the QA officer according to the SOP for line
clearance.
 Take the containers of the product to the packing area. Ensure and check status label
on the product container with correct batch number, batch size and Approved for
packing QC label.
 Start packing according to pack size given.

13.0 Sampling Criteria / Testing Parameters

Mentioned below are the steps after which samples have to be taken and tests are to be
performed according to requirement:
 After final blending Process
 After Compression
 After Coating

14.0 Quality Control Specifications

1 Description

Weight Variation
2
±7.5%
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
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DESVEL 50MG TABLET

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3 Disintegration Time

4 Dissolution

5 Assay (Desvenlafaxine)

6 Uniformity of Dosage Unit

15.0 Assay Results After Final Blending:

BATCH# T-001

ASSAY RESULTS AFTER FINAL BLENDING OF GRANULES

ASSAY= 95 %-105 %
1 2 3
TOP MID BOTTOM

BATCH# T-002

ASSAY RESULTS AFTER FINAL BLENDING OF GRANULES

ASSAY= 95 %-105 %
1 2 3
TOP MID BOTTOM

BATCH# T-003

ASSAY RESULTS AFTER FINAL BLENDING OF GRANULES

ASSAY= 95 %-105 %
1 2 3
TOP MID BOTTOM
 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
PROTOCOL OF PRODUCT
VAL-FM-003 17-12-2019
DESVEL 50MG TABLET

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16.0 Final Report

______________________________________________________________________________
______________________________________________________________________________
______________________________________________________________________________
______________________________________________________________________________

17.0 Recommendation

BMR to be updated

BMR not to be updated

18.0 Outstanding point

______________________________________________________________________________
______________________________________________________________________________
______________________________________________________________________________
______________________________________________________________________________

19.0 Decision:

______________________________________________________________________________
______________________________________________________________________________
______________________________________________________________________________
______________________________________________________________________________

20.0 Report Approval

 MEDISURE LABORATORIES PAKISTAN (Pvt.) Ltd

PROCESS VALIDATION
Ref. Procedure: Revision:00 Date:
PROTOCOL OF PRODUCT
VAL-FM-003 17-12-2019
DESVEL 50MG TABLET

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S.No Name Designation Signature

1 Mr. Sufyan Ullah Assistant Manager

Quality control

Sr Manager
2 Mr. Usman Baig
Production

3 Mr. Anjum Siddiqui Manager QA